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Microwave homogeneous hydrothermal synthesis method of magnesium-aluminum hydrotalcite

A homogeneous hydrothermal and hydrotalcite technology, applied in the direction of alumina/hydroxide, etc., can solve the problem of uneven particle size of hydrotalcite, and achieve the effect of simple operation, high reproducibility, and high uniformity of product particle size

Inactive Publication Date: 2017-01-04
INTEGRATED TECHNICAL SERVICE CENT OF FUQING ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the problem of uneven particle size caused by the current co-precipitation method combined with microwave irradiation method to synthesize hydrotalcite, the purpose of the present invention is to establish a new hydrotalcite synthesis method on the basis of homogeneous precipitation method and microwave irradiation method: microwave uniformity phase hydrothermal synthesis

Method used

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  • Microwave homogeneous hydrothermal synthesis method of magnesium-aluminum hydrotalcite

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Experimental program
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Effect test

Embodiment 1

[0061] (1) Weighing: Weigh 0.03mol of magnesium nitrate hexahydrate, 0.01mol of aluminum nitrate nonahydrate, and 0.18mol of urea;

[0062] (2) Dissolving and subpackaging: Dissolve magnesium nitrate, aluminum nitrate and urea in 100mL deionized water at room temperature, divide into two equal parts, install them in microwave digestion tanks, and seal them;

[0063] (3) Microwave homogeneous hydrothermal synthesis: place the microwave digestion tank in a microwave digestion apparatus, and heat at a set temperature of 130°C for 20 minutes to complete the synthesis;

[0064] (4) Washing and drying: Pour out all the solids and liquids in the microwave tank, wash with deionized water and absolute ethanol respectively, dry in vacuum at 105° C., grind and store.

[0065] From the characterization results of the synthesized magnesium-aluminum hydrotalcite, it can be seen that, figure 1 The three diffraction peaks of X-ray 003, 006, and 009 in X-ray have a multiple relationship, indi...

Embodiment 2

[0067] (1) Weighing: Weigh 0.03mol of magnesium nitrate hexahydrate, 0.01mol of aluminum nitrate nonahydrate, and 0.36mol of urea;

[0068] (2) Dissolving and subpackaging: Dissolve magnesium nitrate, aluminum nitrate and urea in 100mL deionized water at room temperature, divide into two equal parts, install them in microwave digestion tanks, and seal them;

[0069] (3) Microwave homogeneous hydrothermal synthesis: place the microwave digestion tank in a microwave digestion apparatus, and heat at a set temperature of 150°C for 60 minutes to complete the synthesis;

[0070] (4) Washing and drying: Pour out all the solids and liquids in the microwave tank, wash with deionized water and absolute ethanol, dry under vacuum at 105°C, grind and store.

[0071] From the characterization results of the synthesized magnesium-aluminum hydrotalcite, it can be seen that, Figure 5 The three diffraction peaks of X-ray 003, 006, and 009 in X-ray have a multiple relationship, indicating that...

Embodiment 3

[0073] (1) Weighing: Weigh 0.03mol of magnesium nitrate hexahydrate, 0.01mol of aluminum nitrate nonahydrate, and 0.27mol of urea;

[0074] (2) Dissolving and subpackaging: Dissolve magnesium nitrate, aluminum nitrate and urea in 100mL deionized water at room temperature, divide into two equal parts, install them in microwave digestion tanks, and seal them;

[0075] (3) Microwave homogeneous hydrothermal synthesis: place the microwave digestion tank in a microwave digestion apparatus, and heat at a set temperature of 140°C for 40 minutes to complete the synthesis;

[0076] (4) Washing and drying: Pour out all the solids and liquids in the microwave tank, wash with deionized water and absolute ethanol, dry under vacuum at 105°C, grind and store.

[0077] From the characterization results of the synthesized magnesium-aluminum hydrotalcite, it can be seen that, Figure 9 The three diffraction peaks of X-ray 003, 006, and 009 in X-ray have a multiple relationship, indicating that...

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Abstract

The invention belongs to the field of preparation of inorganic materials, and particularly relates to a microwave homogeneous hydrothermal synthesis method of magnesium-aluminum hydrotalcite. The method comprises the following steps: weighing soluble magnesium nitrate, aluminum nitrate and urea according to a certain ratio, and dissolving in deionized water; subpackaging the solution in a microwave digestion tank, sealing, putting in a microwave digestion instrument, and performing microwave heating at a set temperature for a set time to quickly finish synthesis; and pouring out all solids and liquids in the microwave tank, washing with deionized water and anhydrous ethanol, performing vacuum drying, grinding, and storing. By adopting microwave radiation heating, the method provided by the invention has the characteristics of energy saving and high efficiency, can realize temperature and pressure on-line control, and has the advantages of high reproducibility and operational safety; meanwhile, the method does not need pH regulation, and is simple to operate; and the product is high in particle size uniformity. In general, the microwave homogeneous hydrothermal synthesis method established by the invention has the characteristic of being simple, quick and efficient to operate, and is a laboratory method for quickly synthesizing magnesium-aluminum hydrotalcite of a uniform particle size.

Description

technical field [0001] The invention belongs to the technical field of inorganic material preparation, and relates to a microwave homogeneous hydrothermal synthesis method of magnesium-aluminum hydrotalcite. Background technique [0002] Layered double hydroxides (Layered Double Hydroxides, LDHS), also known as layered hydrotalcite, is a typical anionic layered material, and the typical representative is magnesium aluminum hydrotalcite (Mg 6 al 2 (OH) 16 CO 3 4H 2 O), wherein the hydroxide of magnesium and aluminum forms the laminate, and the carbonate ion is an anion between the laminates. Hydrotalcite-like compounds have the characteristics of the controllability of the hydroxide composition of the laminate, the controllability of the type and quantity of interlayer anions, and the controllability of the grain size and distribution; at the same time, this type of material has the characteristics of small size effect, surface effect and Macroscopic quantum tunneling ef...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/02
CPCC01F7/02C01P2002/22C01P2002/72C01P2002/82C01P2004/03C01P2004/61
Inventor 丁立平蔡春平陈学灿刘正才
Owner INTEGRATED TECHNICAL SERVICE CENT OF FUQING ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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